Preparation of pure selenium oxychloride



- chlorid 'upon selenium oxid. The crude oxy colored.

Patented May 1, 192 3.

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GAIL J. PINK, 0]? NIAGARA FALLS, NEW YORK, AND EDMUND DUNCAN GIAUQUE, OF NIAGARA FALLS, ONTARIO, CANADA, ASSIGNORS TO HOOKER ELECTROGEEHIICAL COMPANY, OF NEW YORK, N. Y., A CORPORATION OF NEW YORK.

' PREPARATION or PURE summon oxYonLonrnn.

No Drawing.

To all whom it may concern:

Be it known that we, \(1) GAIL J. FINE and (2) EDMUND DUNCAN GIAUQU'E, citizens of (l) the United States and (2) the United States, residing at (l) Niagara Falls, (2) Niagara Falls, in the county of (1) Niagara, (2) Province of Ontario, and State of (1) New York, (2) Dominion of Canada, have invented certain new and useful Improvements ill the Preparation of Pure Selenium Oxychloride, of which the following is a specification. I

This invention is a novel method whereby commercially pure and light-colored selenium oxychloride may be obtained form impure starting materials, the latter comprising either crude selenium oxychloride, or an impure selenium-bearing material such as a mixture of" crude selenium and seleniunr oxid. i

Selenium oxychloride is a volatile liquid of pale yellow color, which is ordinarily prepared by the reaction of selenium tetrachloride is red or. brown in color, being contaminated by dark colored chlorids of sele-. Ilium. The isolation of the substantially pure oxychloride by fractional distillation at normal or reduced pressures is diflicult if not impossible, the fractions or certain of the fractions being almost invariably dis- This discoloration is attributed principally to selenium monochlorid, which is one of the products of decomposition of selenium oxychlorideunder the distilling conditions, and which has a vapor tension .above that of the oxychloride and therefore imparts its red or brown color to the dis tillate.- ,i

According to our researches, selenium oxychloride tends, at the distilling temperature.

under normal or lower pressures, to undergo decomposition yielding a complex of which the principal components appear to be solenium monochlorid, selenium tetrachlorid, selenium oxid and chlorin. While the exactcomposition of the mixture will of course vary according to the particular equilibrium Application filed January 27, 1921. Serial. K0, 440,494.

conditions, the changes involved may per haps be indicated as follows: 4SeOCI T QSeO +QSeCI S distilling process, or in any other desired way, as for example, by carrying out the distillation in a chlorin atmosphere. By so proceeding, li ht-colored commercially pure seleniumoxyc loride may be'prepared in a single operation from'the crude and discol ored initial product. Any free chlorin dissolved in the distillate may be readily removed, for example by passing through it a current of air or other inert gas.

As a modification of the invention we are able to prepare a 1i ght-colored seleniuni ox-ycliloi'ide by direct distillation from the vessel or reactor in which crude, selenium bearingj materials (preferably amixture of selenium and selen um and in a bath of selenium oxychloride) are caused to react with chlorin, the precaution being observed to maintain an excess of chlorin during the'reaction and also during the distillation which accompanies or follows the' reaction. 1

lVe claim Y 1. Method of refining crude selenium oxychloride which consists in distilling the same in an atmosphere containing an. excess of chlorin.

2. Method of preparing light-coloredse leniuni oxychloride, from crude raivmaterials, comprising reacting with ClllOllIlOli a crude selenium-bearing material and distilling the product in an atmosphere con 'taining an excess of chlorin.

=In testimony whereof, we afiix our signer tures. v

GAIL J. Fina. 

